Preparation method of carboxylic ester compounds

An ester compound and compound technology, applied in the field of compound synthesis, can solve the problems of low catalyst activity, reduced production capacity, difficult to handle, etc., and achieve the effects of high catalyst activity, reduced environmental protection pressure, and less side reactions

Pending Publication Date: 2020-05-08
SHANDONG WEIFANG RAINBOW CHEM
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  • Abstract
  • Description
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Problems solved by technology

[0004] In the above process, the addition process uses cuprous chloride and ethanolamine, the catalyst activity is low, and the reaction time is as long as 20 hours. After the addition reaction is completed, the catalyst needs to be settled and recovered. The standing time is as long as 8 hours, which seriously reduces the production capacity.
In addition, this process will also produce a large amount of cuprous chloride heavy metal waste salt, which is difficult to handle

Method used

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  • Preparation method of carboxylic ester compounds
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  • Preparation method of carboxylic ester compounds

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preparation example Construction

[0026] The invention provides a kind of preparation method of carboxylate compound, comprises the following steps:

[0027] a) Under the action of a catalyst, the compound of the formula (A) and the compound of the formula (B) react to obtain a carboxylate compound of the structure shown in the formula (C);

[0028]

[0029]

[0030] In formula (A)~(C), R 1 from C 1 ~C 2 Alkyl, R 2 ~R 5 independently selected from hydrogen, halogen, C 1 ~C 3 Alkyl or C 1 ~C 3 Haloalkyl;

[0031] The catalysts include azobisisobutyronitrile and / or peroxygen catalysts.

[0032] In the preparation method provided by the present invention, the structural compound of formula (A) and the structural compound of formula (B) are used as reaction raw materials. Wherein, R in the compound of the formula (A) structure 1 The group is a methyl group or an ethyl group, that is, the compound of the formula (A) can specifically be methyl pyritinate or ethyl pyritinate; R in the compound of the...

Embodiment 1

[0045] Carboxylate compounds are synthesized according to the following chemical equation:

[0046]

[0047] The specific process includes:

[0048] 1) Under the protection of nitrogen, add 145.1g methyl peroxyneodecanoate to a 500ml autoclave, close the autoclave, heat up to 60°C, pump 0.71g tert-butyl peroxyneodecanoate and 283.4g trifluoro The trichloroethane mixture was pumped in after 2 hours. Continue to keep warm for 4h.

[0049] 2) Cool down to 30°C, transfer the reaction solution to a four-necked flask, and recover excess trifluorotrichloroethane under reduced pressure to obtain 330.2 g of the product, which was analyzed by GC with a product content of 99.0% and a yield of 99.2%.

[0050] Gas chromatography and mass spectrometry are carried out to the product prepared in this embodiment, wherein the chromatographic analysis results are as follows: figure 1 and as shown in Table 1, figure 1 It is the chromatogram that the embodiment of the present invention 1 pr...

Embodiment 2

[0054] Carboxylate compounds are synthesized according to the following chemical equation:

[0055]

[0056] The specific process includes:

[0057] 1) Under the protection of nitrogen, add 156.2g of ethyl bentinate to a 500ml autoclave, close the autoclave, heat up to 40°C, pump 2.84g of azobisisobutyronitrile and 169.5g of dichloromethane through the feeding port to mix liquid, pumping ends after 2h. Continue to keep warm for 4h.

[0058] 2) Cool down to 30° C., transfer the reaction solution to a four-neck flask, and recover excess methylene chloride under reduced pressure to obtain 241.2 g of product. GC analysis shows that the product content is 98.0%, and the yield is 98.1%.

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Abstract

The invention belongs to the technical field of compound synthesis, and particularly relates to a preparation method of carboxylic ester compounds. A compound having a structure represented by formula(A) reacts with a compound having a structure represented by formula (B) under the action of a catalyst to obtain the carboxylic ester compounds having a structure represented by formula (C); in theformulas (A)-(C), R1 is selected from C1-C2 alkyl groups; R2 to R5 are independently selected from hydrogen, halogen, C1-3 alkyl groups or C1-3 halogenated alkyl groups; and the catalyst comprises azodiisobutyronitrile and / or a peroxide catalyst. The compound of formula (A) and the compound of formula (B) are used as reaction raw materials and directly react under the action of the specific catalyst to obtain the carboxylic ester compounds. The method has the advantages of high catalytic activity, simple process flow, low post-treatment difficulty and high production efficiency, can avoid thegeneration of three wastes, and conforms to the environmental protection requirements.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a preparation method of carboxylic acid ester compounds. Background technique [0002] Halogen-3,3-dimethyl-heptane carboxylate compounds are synthetic compounds of lambda-cyhalothrin, tefluthrin, resmethrin, phenothrin, permethrin, cypermethrin, bromemethrin Important intermediates of pyrethroids such as permethrin and tetrabromothrin. The global sales of pyrethroid products rose rapidly from US$2.08 billion in 2009 to US$3.16 billion in 2014, with a compound annual growth rate of 8.7%. From the perspective of the distribution of global insecticide products, the market share of pyrethroids is 17.0%, second only to neonicotinoid insecticides. From the perspective of the scale distribution of permethrin products, in 2015, the global sales volume was mainly agricultural permethrin, among which the sales of beta-cyhalothrin (Kung Fu permethrin) reached 630 m...

Claims

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Application Information

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IPC IPC(8): C07C67/307C07C69/63
CPCC07C67/307C07C69/63Y02P20/584
Inventor 李志清绳敏姚红霞徐安
Owner SHANDONG WEIFANG RAINBOW CHEM
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